WO2013094613A1 - 熱伝導性シート及び熱伝導性シートの製造方法 - Google Patents

熱伝導性シート及び熱伝導性シートの製造方法 Download PDF

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Publication number
WO2013094613A1
WO2013094613A1 PCT/JP2012/082817 JP2012082817W WO2013094613A1 WO 2013094613 A1 WO2013094613 A1 WO 2013094613A1 JP 2012082817 W JP2012082817 W JP 2012082817W WO 2013094613 A1 WO2013094613 A1 WO 2013094613A1
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Prior art keywords
conductive sheet
filler
thermally conductive
heat conductive
thermal
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PCT/JP2012/082817
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English (en)
French (fr)
Japanese (ja)
Inventor
荒巻 慶輔
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デクセリアルズ株式会社
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Priority to CN201280061296.7A priority Critical patent/CN103975429B/zh
Publication of WO2013094613A1 publication Critical patent/WO2013094613A1/ja

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/34Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3737Organic materials with or without a thermoconductive filler
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00Compositions of unspecified macromolecular compounds
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00Constructional details common to different types of electric apparatus
    • H05K7/20Modifications to facilitate cooling, ventilating, or heating
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001Technical content checked by a classifier
    • H01L2924/0002Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the present invention relates to a heat conductive sheet that promotes heat dissipation from a heat-generating electronic component and the like, and a method for manufacturing the heat conductive sheet.
  • the semiconductor is attached to a heat sink such as a heat dissipating fan or a heat dissipating plate via a heat conductive sheet.
  • a heat conductive sheet a sheet in which a filler such as an inorganic filler is dispersed and contained in silicone is widely used.
  • further improvement in thermal conductivity is required, and in general, for the purpose of high thermal conductivity, it is possible to respond by increasing the filling rate of the inorganic filler mixed in the matrix. Yes.
  • the filling rate of the inorganic filler is increased, flexibility is impaired, or powder falling occurs because the filling rate of the inorganic filler is high, so there is a limit to increasing the filling rate of the inorganic filler.
  • the inorganic filler examples include alumina, aluminum nitride, and aluminum hydroxide.
  • scale-like particles such as boron nitride and graphite, carbon fibers, and the like may be filled in the matrix. This is due to the anisotropy of the thermal conductivity of the scaly particles.
  • carbon fiber has a thermal conductivity of about 600 to 1200 W / mK in the fiber direction.
  • Boron nitride has a thermal conductivity of about 110 W / mK in the plane direction and about 2 W / mK in a direction perpendicular to the plane direction, and is known to have anisotropy. .
  • the thermal conductivity of a thermally conductive sheet is improved when the filling amount of the thermally conductive filler is increased.
  • the fibrous heat conductive filler cannot increase the filling amount as compared with the spherical filler. Therefore, high thermal conductivity cannot be obtained with the fibrous thermal conductive filler alone.
  • the surface direction of the fibrous heat conductive filler is made the same as the thickness direction of the heat conductive sheet, which is the heat transfer direction, that is, the fibrous heat conductive filler is arranged in the thickness direction of the heat conductive sheet. By orienting, the thermal conductivity can be dramatically improved.
  • Patent Document 1 describes a method of applying a heat conductive composition containing carbon fiber and orienting the carbon fiber by applying a magnetic field. However, since fluidity is required for the orientation of the carbon fibers, the method described in Patent Document 1 cannot increase the filling amount of the heat conductive filler. Therefore, a heat conductive sheet is desired in which the heat conductive filler is oriented along the thickness direction of the heat conductive sheet and the heat conductivity in the thickness direction is good.
  • This invention is proposed in view of such a situation, and it aims at providing the manufacturing method of the heat conductive sheet with favorable heat conductivity of the thickness direction, and a heat conductive sheet.
  • the present inventor has expressed the “L *” value in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” when the surface of the heat conductive sheet is measured. It was found that there is a high correlation between the brightness L * and the thermal conductivity, and the present invention has been completed.
  • the present invention relates to a thermally conductive sheet comprising a thermally conductive composition containing a curable resin composition and a filler that aligns the thermally conductive filler in a predetermined direction, wherein the thermally conductive filler is thermally conductive.
  • the lightness L * represented by the “L *” value in the b color system is 32.5 or more.
  • the manufacturing method of the heat conductive sheet which concerns on this invention produces the heat conductive composition containing the curable resin composition, the heat conductive filler, and the filler which aligns a heat conductive filler in a predetermined direction.
  • JIS Z 8729 and “JIS Z 8730” as measured when the surface of the thermally conductive sheet is measured and the surface of the thermally conductive sheet is oriented along the thickness direction of the thermally conductive sheet and contains at least aluminum nitride.
  • the L * a * b Table lightness represented by "L *" value in the color scheme L * is 32.5 or more.
  • the thermal conductivity evaluation method includes a thermally conductive composition containing a curable resin composition, a thermally conductive filler, and a filler that aligns the thermally conductive filler in a predetermined direction.
  • the lightness L * represented by the “L *” value in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” when measuring the surface of the conductive sheet
  • the thermal conductivity of the sheet is evaluated.
  • the thermal conductive filler is oriented along the thickness direction of the thermal conductive sheet, and includes at least aluminum nitride as a filler.
  • the heat conductive filler is oriented along the thickness direction of the heat conductive sheet, and the heat in the thickness direction of the heat conductive sheet is The conductivity can be improved.
  • FIG. 1 is a flowchart for explaining an example of a method for producing a thermally conductive sheet according to the present invention.
  • FIG. 2 is an external view showing an example of an ultrasonic cutting machine used in a cutting step in the method for producing a thermally conductive sheet according to the present invention.
  • FIG. 3 is an external view showing an example of a slicing apparatus.
  • FIG. 4 is a flowchart for explaining an example of the arranging step in the method for producing another thermally conductive sheet according to the present invention.
  • Drawing 5 is a mimetic diagram for explaining an example of a temporary forming process, an alignment process, and a main forming process in a manufacturing method of a heat conductive sheet concerning the present invention.
  • FIG. 1 is a flowchart for explaining an example of a method for producing a thermally conductive sheet according to the present invention.
  • FIG. 2 is an external view showing an example of an ultrasonic cutting machine used in a cutting step in the method for producing a thermally conductive
  • FIG. 6 is a perspective view showing an example of a laminate obtained in the alignment step in the method for manufacturing a heat conductive sheet according to the present invention.
  • FIG. 7A is a perspective view showing an example of the molded body that has not been pressed, and
  • FIG. 7B is a perspective view showing an example of the molded body that has been pressed.
  • the thermally conductive sheet 1 includes a thermally conductive composition containing a curable resin composition, a thermally conductive filler, and a filler that aligns the thermally conductive filler in a predetermined direction.
  • the heat conductive filler is oriented along the thickness direction of the heat conductive sheet.
  • the thermally conductive sheet according to the present embodiment includes at least aluminum nitride in the thermally conductive sheet, and described in “JIS Z 8729” and “JIS Z 8730” when the surface of the thermally conductive sheet is measured.
  • the lightness L * represented by the “L *” value in the L * a * b color system is 32.5 or more.
  • the thermally conductive filler is oriented along the thickness direction of the thermally conductive sheet, and the thickness direction of the thermally conductive sheet is Thermal conductivity can be improved.
  • the color of an object generally consists of three elements: lightness (brightness), hue (hue), and saturation (brightness).
  • lightness (brightness), hue (hue), and saturation (brightness).
  • hue (hue)
  • saturation (brightness).
  • a color system that expresses these numerically objectively is necessary.
  • An example of such a color system is the L * a * b color system.
  • the L * a * b color system can be easily measured by a measuring instrument such as a commercially available spectrophotometer.
  • the L * a * b color system is a color system described in “JIS Z 8729” and “JIS Z 8730”, for example, and is shown by arranging each color in a spherical color space.
  • lightness is indicated by a position in the vertical axis (z-axis) direction
  • hue is indicated by a position in the outer peripheral direction
  • saturation is indicated by a distance from the central axis.
  • the position in the vertical axis (z-axis) direction indicating brightness is indicated by L *.
  • the value of the lightness L * is a positive number. The smaller the number, the lower the lightness and the darker the tendency. Specifically, the value of L * varies from 0 corresponding to black to 100 corresponding to white.
  • the positive direction of the x axis is the red direction
  • the positive direction of the y axis is the yellow direction
  • the negative direction of the x axis is the green direction
  • y The negative direction of the axis is the blue direction.
  • the position in the x-axis direction is represented by a * taking a value from ⁇ 60 to +60.
  • the position in the y-axis direction is represented by b * taking values from ⁇ 60 to +60.
  • a * and b * are positive and negative numbers representing chromaticity, and the closer to 0, the blacker the color becomes. Hue and saturation are represented by these a * and b * values.
  • the color becomes green when a * is less than ⁇ 1 and the color becomes red when a * is ⁇ 1 or more.
  • the color becomes bluish, and when b * exceeds +1, the color becomes yellow.
  • the lightness L * when it becomes 32.5 or more, it becomes whitish. This is because when the lightness L * is 32.5 or more, when the heat conductive sheet is observed from the direction perpendicular to the cut surface, the area of the heat conductive filler in the heat conductive sheet decreases, This is because white alumina and aluminum nitride are exposed on the surface of the heat conductive sheet. That is, when the lightness L * is 32.5 or more, it means that the thermally conductive filler is oriented along the thickness direction of the thermally conductive sheet.
  • the lightness L was obtained when the cross section of the heat conductive sheet containing carbon fiber as the heat conductive filler and containing aluminum nitride and alumina as the filler was used. When it becomes less than 32.5, it becomes dark. This is because when the lightness L * is less than 32.5, when the thermally conductive sheet is observed from a direction perpendicular to the cut surface, the area of the thermally conductive filler in the thermally conductive sheet increases, This is because white alumina and aluminum nitride are not easily exposed from the surface of the heat conductive sheet. That is, when the lightness L * is less than 32.5, it means that the heat conductive filler is not oriented along the thickness direction of the heat conductive sheet, compared to when the lightness L * is 32.5 or more. .
  • the thermal conductivity of the thermally conductive sheet is improved.
  • the thermal conductivity is improved when a large amount of pitch-based carbon fibers, for example, is filled as the thermally conductive filler. That is, it is considered that the thermal conductivity is improved when the lightness L * on the surface of the thermal conductive sheet is reduced.
  • the viscosity of the thermally conductive composition at the time of extrusion is not only increased by adding the content of the thermally conductive filler, but also by maintaining the shape by adding a filler. It is important to orient the heat conductive filler along the thickness direction of the heat conductive sheet.
  • the present inventor has expressed the “L *” value in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” when the surface of the heat conductive sheet is measured. It was found that there is a high correlation between the brightness L * and the thermal conductivity. Moreover, in order to orient the heat conductive filler along the thickness direction of the heat conductive sheet, the amount of aluminum nitride having a lower thermal conductivity than the heat conductive filler is less than the amount of heat conductive filler. I found that it has a big influence.
  • At least aluminum nitride is contained in the heat conductive sheet, and the lightness L * when the surface of the heat conductive sheet is measured is set to 32.5 or more, whereby the heat conductive filler is in the thickness direction of the heat conductive sheet.
  • the thermal conductivity in the thickness direction of the thermal conductive sheet can be improved.
  • the curable resin composition contained in the heat conductive sheet is not particularly limited, and for example, a silicone-based adhesive, an acrylic resin-based adhesive, or the like is used.
  • a silicone-based adhesive a condensation curable type or an addition curable type can be used.
  • the content of the curable resin composition is not particularly limited, and can be, for example, 25 to 45% by volume.
  • thermally conductive filler for example, carbon fibers can be used, and it is particularly preferable to use pitch-based carbon fibers.
  • Pitch-based carbon fibers are made from pitch as a main raw material and graphitized by heat treatment at a high temperature exceeding 2000 to 3000 ° C. or 3000 ° C. after each processing step such as melt spinning, infusibilization and carbonization.
  • the raw material pitch is divided into an isotropic pitch that is optically disordered and does not exhibit deflection, and an anisotropic pitch (mesophase pitch) in which constituent molecules are arranged in a liquid crystal form and exhibit optical anisotropy.
  • Carbon fibers manufactured from anisotropic pitch have better mechanical properties than carbon fibers manufactured from isotropic pitch, and electrical and thermal conductivity is increased. Therefore, it is preferable to use a mesophase pitch graphitized carbon fiber.
  • the average fiber length of the heat conductive filler is preferably 100 ⁇ m or more. By setting the average fiber length of the heat conductive filler to 100 ⁇ m or more, the heat conductive filler can be easily aligned in the same direction, so that the heat conductivity in the thickness direction of the heat conductive sheet can be improved.
  • the content of the heat conductive filler in the heat conductive sheet is preferably 15 to 25% by volume.
  • the content of the heat conductive filler is preferably 15 to 25% by volume.
  • the thermal resistance value can be more effectively lowered, so that the heat conductivity in the thickness direction of the heat conductive sheet can be improved.
  • content of a heat conductive filler shall be 25 volume% or less, when extruding a heat conductive composition with an extruder, it can prevent that extrusion becomes difficult, for example.
  • the filler makes it easy to align the thermally conductive filler in a predetermined direction due to the difference in flow rate from the thermally conductive filler in the thermally conductive composition, that is, the thermally conductive filler is thermally conductive along the extrusion direction. It is used to facilitate the orientation of the filler.
  • the filler is also used to function as a heat conductive material.
  • the filler for example, alumina, aluminum nitride, boron nitride, zinc oxide, silicon powder, metal powder can be used, and at least aluminum nitride is used.
  • Aluminum nitride has nitrogen in the molecule, and this nitrogen inhibits the reaction of the curable resin composition and suppresses the increase in the viscosity of the thermally conductive composition. Therefore, by using at least aluminum nitride as the filler, the heat conductive filler is more effectively placed in a predetermined direction, that is, the thickness of the heat conductive sheet, compared to when only alumina particles are used as the filler. It can be oriented along the direction. Therefore, since at least aluminum nitride is used as the filler, the thermally conductive filler can be more effectively oriented along the thickness direction of the thermally conductive sheet. Property can be improved.
  • the thermally conductive filler is oriented along the thickness direction of the thermally conductive sheet by using two or more kinds of spherical particles having different particle diameters as the filler, the thickness direction of the thermally conductive sheet The thermal conductivity of can be made better.
  • the content of the filler in the heat conductive sheet is preferably 40 to 50% by volume. Moreover, it is preferable to contain 5.1 volume% or more of aluminum nitride in a heat conductive sheet. By making the content of aluminum nitride in the thermally conductive sheet 5.1 volume% or more, the increase in the viscosity of the thermally conductive composition is effectively suppressed, and the thermally conductive filler is more effectively thermally conducted. Can be oriented along the thickness direction of the adhesive sheet.
  • the brightness L * represented by the “L *” value in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” when the surface of the heat conductive sheet was measured It can be more effectively 32.5 or more.
  • the heat conductivity of the thickness direction of a conductive sheet can be made more favorable by content of aluminum nitride in a heat conductive sheet being 5.1 volume% or more.
  • the average particle diameter of the filler is preferably 0.5 to 5 ⁇ m. By setting the average particle size of the filler to 0.5 ⁇ m or more and 5 ⁇ m or less, it functions sufficiently as a thermally conductive material, and the orientation of the thermally conductive filler is less likely to be disturbed in the thermally conductive composition.
  • the thermal conductivity in the thickness direction of the thermal conductive sheet 1 can be made better.
  • the large spherical particles may be 2 to 5 ⁇ m and the small spherical particles may be 0.3 to 2 ⁇ m. preferable.
  • the brightness L * represented by the “L *” value in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” when the surface of the heat conductive sheet is measured It can be surely 32.5 or more.
  • the L * a * b color system is taken as an example, but the method of selecting the color system is not particularly limited, and a table that can be converted into the L * a * b color system. Any color system may be used. For example, an XYZ color system or an L * C * h color system may be used.
  • the heat conductive sheet 1 mentioned above can be produced by the following manufacturing method, for example.
  • the manufacturing method of the heat conductive sheet which concerns on this Embodiment has heat conductive composition preparation process S1, orientation process S2, and cutting process S3, as shown in FIG.
  • Thermal conductive composition creation step S1 In heat conductive composition creation process S1, the heat conductive composition mentioned above is created.
  • the blending amount in the heat conductive composition is preferably, for example, 15 to 25% by volume of the heat conductive filler and 40 to 50% by volume of the filler.
  • the thermally conductive composition created in the thermally conductive composition creating step S1 is formed in a columnar shape, and the thermally conductive filler is oriented in the columnar longitudinal direction.
  • a columnar heat conductive composition in which the heat conductive filler is aligned in the columnar longitudinal direction L as shown in FIG. Article 2 can be formed.
  • the heat conductive composition prepared in the heat conductive composition preparation step S1 is applied onto a polyester film coated with a release material, and the columnar heat conduction as shown in FIG. The composition 2 may be formed.
  • the columnar thermal conductivity in the direction V perpendicular to the longitudinal direction L of the columnar thermal conductive composition 2 using an ultrasonic cutter 3 is used.
  • the thermally conductive sheet 1 can be formed while maintaining the orientation of the thermally conductive filler. Therefore, the orientation of the heat conductive filler is maintained in the thickness direction, and the heat conductive sheet 1 having good heat conduction characteristics can be obtained.
  • the ultrasonic cutting machine 3 includes a work table 5 on which the columnar heat conductive composition 2 is placed, and a columnar heat conductive composition on the work table 5 while applying ultrasonic vibration. And an ultrasonic cutter 4 for slicing 2.
  • the work table 5 is provided with a silicone rubber 7 on a metal moving table 6.
  • the moving table 6 can be moved in a predetermined direction by the moving mechanism 8, and sequentially feeds the columnar heat conductive composition 2 to the lower part of the ultrasonic cutter 4.
  • the silicone rubber 7 has a thickness sufficient to receive the cutting edge of the ultrasonic cutter 4.
  • the ultrasonic cutter 4 has a knife 9 for slicing the columnar thermal conductive composition 2, an ultrasonic oscillation mechanism 10 for applying ultrasonic vibration to the knife 9, and an elevating mechanism 11 for raising and lowering the knife 9.
  • the knife 9 has its cutting edge directed toward the work table 5 and is moved up and down by the elevating mechanism 11 to slice the columnar thermal conductive composition 2 placed on the work table 5.
  • the dimensions and material of the knife 9 are determined according to the size and composition of the columnar heat conductive composition 2.
  • the knife 9 is made of steel having a width of 40 mm, a thickness of 1.5 mm, and a cutting edge angle of 10 °.
  • the ultrasonic oscillation mechanism 10 applies ultrasonic vibration to the knife 9 in the slicing direction of the columnar thermal conductive composition 2.
  • the transmission frequency is 20.5 kHz
  • the amplitude is 50 ⁇ m, 60 ⁇ m
  • Adjustment is possible in three stages of 70 ⁇ m.
  • Such an ultrasonic cutting machine 3 slices the columnar thermal conductive composition 2 while applying ultrasonic vibration to the ultrasonic cutter 4, thereby aligning the thermal conductive filler of the thermal conductive sheet 1. Can be maintained in the thickness direction of the heat conductive sheet 1.
  • the heat conductive sheet 1 sliced while applying ultrasonic vibration by the ultrasonic cutting machine 3 has a lower thermal resistance than the heat conductive sheet sliced without applying ultrasonic vibration. Since the ultrasonic cutter 3 imparts ultrasonic vibration in the slicing direction to the ultrasonic cutter 4, the thermal conductive filler has a low interface thermal resistance and is oriented in the thickness direction of the thermal conductive sheet 1. This is because it is difficult to be laid down by the knife 9. On the other hand, in a thermally conductive sheet sliced without applying ultrasonic vibration, the orientation of the thermally conductive filler is disturbed by the frictional resistance of the knife, and the exposure to the cut surface is reduced, which increases the thermal resistance. End up. Therefore, by using the ultrasonic cutting machine 3, the heat conductive sheet 1 having excellent heat conduction characteristics can be obtained.
  • the heat conductive filler is oriented along the thickness direction of the heat conductive sheet 1 and the surface of the heat conductive sheet 1 is measured.
  • a heat conductive sheet 1 having a lightness L * of 32.5 or more represented by an “L *” value in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” can be obtained. .
  • the alignment step S ⁇ b> 2 of the above-described method for manufacturing a heat conductive sheet may include a temporary molding step S ⁇ b> 21, an alignment step S ⁇ b> 22, and a main molding step S ⁇ b> 23.
  • the heat conductive sheet 1 having a lightness L * represented by a value of “*” of 32.5 or more can be obtained more reliably.
  • the heat conductive fillers in the heat conductive sheet 1 can be more reliably aligned in the same direction, and the heat conductivity in the thickness direction of the heat conductive sheet 1 can be further improved.
  • the detailed description is abbreviate
  • Temporal molding process S21 In temporary molding process S21, as shown to FIG. 5 (A), the heat conductive composition 12 created by heat conductive composition preparation process S1 is extruded with the extruder 13, and a heat conductive filler is followed along an extrusion direction.
  • a long columnar temporary molded body 14 (hereinafter referred to as a temporary molded body 14) in which is oriented.
  • the extruder 13 is configured in an elongated cylindrical shape, and the diameter W2 of the opening 12B on the side from which the heat conductive composition 12 is discharged is the main body portion. It is preferable that the diameter is smaller than the inner diameter W1 of 12A. Further, in the extruder 13, the inner diameter W1 of the main body 12A is reduced in a taper shape from a predetermined position in the longitudinal direction toward the extrusion direction, and the aperture W2 of the opening 12B is larger than the inner diameter W1 of the main body 12A. The diameter may be reduced.
  • the heat conductive filler is easily along the extrusion direction. Thereby, a heat conductive filler can be more reliably orientated in the longitudinal direction of the temporary molding 14.
  • the diameter W2 of the opening 12B is set to about 1.5 to 9.5 mm. Is preferred. In this case, when the diameter W2 of the opening 12B is set to 1.5 mm or more, it is possible to prevent the extrusion from becoming difficult when the heat conductive composition 12 is extruded by the extruder 13. Moreover, since the orientation of the heat conductive filler is hardly disturbed by setting the diameter W2 of the opening 12B to 9.5 mm or less, the heat conductivity in the thickness direction of the heat conductive sheet 1 can be further improved. it can.
  • the cross-sectional shape of the opening 12B can be, for example, a circular shape, a triangular shape, a rectangular shape, or a square shape, but is preferably a rectangular shape or a square shape.
  • the temporary molded body 14 has a prismatic shape. Therefore, in the alignment step S22, the plurality of temporary molded bodies 14 are aligned so as to be adjacent to the direction orthogonal to the longitudinal direction, and the aligned plurality of temporary molded bodies 14 are arranged in a direction substantially orthogonal to the alignment direction.
  • the laminated body 14A When obtaining the laminated body 14A (hereinafter, referred to as the laminated body 14A), it is difficult to generate a gap between the laminated bodies 14A. Thereby, since it becomes difficult for bubbles to be contained in the laminated body 14A, it is possible to obtain the main molded body 16 having more excellent flame retardancy in the main molding step S23.
  • the temporary molded body 14 has heat conductive fillers oriented along the direction of extrusion by the extruder 13, and has an elongated columnar shape, for example, an elongated square columnar shape, an elongated triangular columnar shape, or an elongated columnar shape.
  • the plurality of temporary molded bodies 14 formed in the temporary molding step S21 are adjacent to each other in the direction orthogonal to the longitudinal direction.
  • the laminated body 14A is obtained.
  • the temporary molded bodies 14 are aligned in a predetermined frame 15, and a laminated body 14A in which the temporary molded bodies 14 are arranged in a rectangular parallelepiped shape or a cubic shape is obtained.
  • the frame 15 is used as a fixing means for fixing the laminated body 14A when the main molded body 16 is molded in the main molding step S23, and prevents the laminated body 14A from being greatly deformed.
  • the frame 15 is made of, for example, metal.
  • the laminated body 14A obtained in the alignment step S22 is cured, so that FIG. 5E, FIG. 7A, and FIG.
  • the molded body 16 in which the temporary molded bodies 14 constituting the laminated body 14A are integrated is molded.
  • the method of curing the laminate 14A include a method of heating the laminate 14A with a heating device and a method of heating and pressurizing the laminate 14A with a heating and pressurizing device.
  • an acrylic resin is used as the curable resin composition constituting the heat conductive composition 12, for example, the laminate 14A is cured at room temperature by including an isocyanate compound in the heat conductive composition 12. It is possible.
  • a method of heating and pressurizing the laminate 14A with a heating and pressurizing device that is, when curing the laminate 14A, a plurality of temporary molded bodies 14 constituting the laminate 14A. It is preferable to press in a direction perpendicular to the longitudinal direction (vertical direction). By pressing the laminated body 14A in this way, air bubbles can be more reliably removed from the laminated body 14A, so that it is possible to obtain the molded body 16 with better flame retardancy in the main molding step S23. It becomes.
  • the main molded body 16 molded in the main molding step S23 is cut into a predetermined dimension by the ultrasonic cutting machine 3 in a direction orthogonal to the longitudinal direction of the temporary molded body 14.
  • the ultrasonic cutting machine 3 slices the molded body 16 into individual heat conductive sheets 1 in order to obtain the heat conductive sheet 1.
  • the main molded body 16 is sliced by the ultrasonic cutter 4 in the direction of the arrow perpendicular to the longitudinal direction of the temporary molded body 14, so that heat conduction is maintained while maintaining the orientation of the thermally conductive filler.
  • the sheet 1 can be formed. Therefore, it is possible to obtain the heat conductive sheet 1 having good heat conduction characteristics in which the orientation of the heat conductive filler is maintained in the thickness direction.
  • the color evaluation method according to the present embodiment is “L” in the L * a * b color system described in “JIS Z 8729” and “JIS Z 8730” when the surface of the above-described heat conductive sheet 1 is measured.
  • the thermal conductivity of the heat conductive sheet 1 is evaluated using the lightness L * represented by the value “*”. For example, when the lightness L * when the surface of the thermal conductive sheet 1 is measured is 32.5 or more, the thermal conductive filler is oriented along the thickness direction of the thermal conductive sheet 1, and thus the thermal conductivity. It can be evaluated that the thermal conductivity in the thickness direction of the sheet 1 is good.
  • the heat conductive filler is not oriented along the thickness direction of the heat conductive sheet 1, and thus the heat conduction. It can be evaluated that the thermal conductivity in the thickness direction of the conductive sheet 1 is not good.
  • thermo conductivity sheets obtained in Examples 1 to 6 and Comparative Examples 1 to 3 were evaluated for the orientation, thermal conductivity, and appearance of pitch-based carbon fibers.
  • Example 1 In Example 1, 24% by volume of alumina particles (filler) (product name: DAW-03, manufactured by Denki Kagaku Kogyo Co., Ltd.) having an average particle size of 3 ⁇ m were added to the two-component addition reaction type liquid silicone resin, and the average particle size Aluminum nitride particles 1 ⁇ m in diameter (manufactured by Tokuyama Co., Ltd.) 18.3% by volume, pitch-based carbon fiber (thermal conductive filler) having an average major axis length of 150 ⁇ m and an average minor axis length of 8 ⁇ m (manufactured by Teijin Limited A silicone resin composition (thermally conductive composition) was prepared by dispersing 24.1% by volume of trade name: Lahima R-A301).
  • the two-component addition reaction type liquid silicone resin is composed of 16.8% by volume of silicone A solution (organopolysiloxane having a vinyl group) and 18.8% by volume of silicone B solution (organopolysiloxane having an H—Si group). Are mixed.
  • the obtained silicone resin composition was extruded into a mold (20 mm ⁇ 20 mm) coated with a release material to mold a silicone molded body.
  • the obtained silicone molding was cured in an oven at 100 ° C. for 1 hour to obtain a silicone cured product.
  • the obtained cured silicone was cut with an ultrasonic cutter so as to have a thickness of 2.0 mm to obtain a thermally conductive sheet having a thickness of 2.0 mm.
  • the slice speed of the ultrasonic cutter was 50 mm per second.
  • the ultrasonic vibration applied to the ultrasonic cutter had an oscillation frequency of 20.5 kHz and an amplitude of 60 ⁇ m.
  • Example 2 In Example 2, alumina particles having an average particle diameter of 3 ⁇ m (electrochemical industry) were added to a two-component addition reaction type liquid silicone resin in which 16.8 vol% of silicone A liquid and 18.8 vol% of silicone B liquid were mixed.
  • Product name: DAW-03 11.7% by volume
  • aluminum nitride particles having an average particle diameter of 1 ⁇ m Tokuyama Co., Ltd.
  • average major axis length 150 ⁇ m average minor axis
  • a silicone resin composition was prepared by dispersing 23.5% by volume of pitch-based carbon fiber (trade name: Lahima R-A301, manufactured by Teijin Limited) having a length of 8 ⁇ m, the same as in Example 1.
  • pitch-based carbon fiber trade name: Lahima R-A301, manufactured by Teijin Limited
  • Example 3 In Example 3, alumina particles having an average particle diameter of 3 ⁇ m (electrochemical industry) were added to a two-component addition reaction type liquid silicone resin in which 18.8% by volume of a silicone A liquid and 18.8% by volume of a silicone B liquid were mixed.
  • Example 4 alumina particles having an average particle diameter of 3 ⁇ m (electrochemical industry) were added to a two-component addition reaction type liquid silicone resin in which 18.8 vol% of silicone A liquid and 18.8 vol% of silicone B liquid were mixed.
  • Product name: DAW-03 28% by volume
  • aluminum nitride particles having an average particle diameter of 1 ⁇ m made by Tokuyama Co., Ltd.
  • 14.3% by volume average major axis length 150 ⁇ m
  • average minor axis length A silicone resin composition was prepared by dispersing 20.1% by volume of 8 ⁇ m pitch-based carbon fiber (trade name: Lahima R-A301, manufactured by Teijin Limited).
  • the obtained silicone resin composition was coated (laminated coating) on a polyester film coated with a release material to prepare a silicone molded body.
  • the obtained silicone molded body was heated in an oven at 100 ° C. for 1 hour to obtain a cured silicone product.
  • the obtained cured silicone was cut with an ultrasonic cutter so as to have a thickness of 2.0 mm to obtain a thermally conductive sheet having a thickness of 2.0 mm.
  • the slice speed of the ultrasonic cutter was 50 mm per second.
  • the ultrasonic vibration applied to the ultrasonic cutter had an oscillation frequency of 20.5 kHz and an amplitude of 60 ⁇ m.
  • Example 5 alumina particles having an average particle diameter of 3 ⁇ m (electrochemical industry) were added to a two-component addition reaction type liquid silicone resin in which 18.8 vol% of silicone A liquid and 18.8 vol% of silicone B liquid were mixed.
  • Product name: DAW-03 37.2% by volume
  • aluminum nitride particles having an average particle diameter of 1 ⁇ m made by Tokuyama Co., Ltd.
  • a silicone resin composition was prepared by dispersing 20.1% by volume of pitch-based carbon fiber (trade name: Lahima R-A301, manufactured by Teijin Ltd.) having a length of 8 ⁇ m.
  • pitch-based carbon fiber trade name: Lahima R-A301, manufactured by Teijin Ltd.
  • Example 6 aluminum nitride particles having an average particle diameter of 1 ⁇ m (inc.) Were added to a two-component addition reaction type liquid silicone resin in which 17.1% by volume of silicone A liquid and 17.1% by volume of silicone B liquid were mixed. 42.6% by volume) and 23.2% by volume of pitch-based carbon fiber having an average major axis length of 150 ⁇ m and an average minor axis length of 8 ⁇ m (manufactured by Teijin Limited, trade name: Lahima R-A301).
  • a thermally conductive sheet was obtained in the same manner as in Example 1 except that the silicone resin composition was prepared by dispersing.
  • Comparative Example 1 alumina particles having an average particle size of 3 ⁇ m (electrochemical industry) were added to a two-component addition reaction type liquid silicone resin in which 18.8 vol% of silicone A liquid and 18.8 vol% of silicone B liquid were mixed.
  • Product name: DAW-03 42.3% by volume
  • pitch-based carbon fiber with an average major axis length of 150 ⁇ m and an average minor axis length of 8 ⁇ m manufactured by Teijin Limited, trade name: Lahima R-A301
  • a thermally conductive sheet was obtained in the same manner as in Example 1 except that 24.1% by volume was dispersed to prepare a silicone resin composition.
  • Comparative Example 2 In Comparative Example 2, alumina particles having an average particle diameter of 3 ⁇ m (electrochemical industry) were added to a two-component addition reaction type liquid silicone resin in which 18.8 vol% of silicone A liquid and 18.8 vol% of silicone B liquid were mixed.
  • Product name: DAW-03 41.3% by volume
  • pitch-based carbon fiber with an average major axis length of 150 ⁇ m and an average minor axis length of 8 ⁇ m manufactured by Teijin Limited, trade name: Lahima R-A301
  • a thermally conductive sheet was obtained in the same manner as in Example 4 except that 20.1% by volume was dispersed to prepare a silicone resin composition.
  • Comparative Example 3 In Comparative Example 3, alumina particles having an average particle diameter of 3 ⁇ m (manufactured by Denki Kagaku Kogyo Co., Ltd.) were added to a two-component addition-reaction type liquid silicone resin in which 18% by volume of silicone A solution and 18% by volume of silicone B solution were mixed.
  • Product name: DAW-03 44.8% by volume
  • pitch-based carbon fiber having an average major axis length of 150 ⁇ m and an average minor axis length of 8 ⁇ m (trade name: Lahima R-A301, manufactured by Teijin Limited), 19.2 volumes % Was dispersed in the same manner as in Example 1 except that a silicone resin composition was prepared.
  • Table 1 shows a summary of conditions and the like of Examples 1 to 6 and Comparative Examples 1 to 3.
  • the orientation of the pitch-based carbon fibers was evaluated by observing the cross section of the thermally conductive sheet with an SEM and measuring the blackness using the L * a * b color system.
  • the pitch-based carbon fibers were oriented with respect to the thickness direction of the heat conductive sheets.
  • the heat conductive sheets obtained in Examples 1 to 3, Example 5 and Example 6 are better in pitch-based carbon fiber than the heat conductive sheets obtained in Example 4.
  • the blackness of the cross section of the heat conductive sheet was measured using the L * a * b color system.
  • a color display method representing the L * a * b color system defined in “JIS Z 8729” was used as an index of blackness.
  • a spectrophotometer product name: CM-700d, manufactured by Konica Minolta Sensing Co., Ltd. was used for measurement of blackness using the L * a * b color system.
  • the heat conductive sheets obtained in Examples 1 to 6 are “L *” values in the L * a * b color system described in “JIS Z 8729” when the surface of the heat conductive sheet is measured.
  • the lightness L * expressed was 32.5 or more.
  • the heat conductive sheets obtained in Comparative Examples 1 to 3 are “L *” in the L * a * b color system described in “JIS Z 8729” when the surface of the heat conductive sheet is measured.
  • the lightness L * represented by the value was less than 32.5. From these results, the heat conductive sheets obtained in Examples 1 to 6 are more effective in pitch-based carbon fibers than the heat conductive sheets obtained in Comparative Examples 1 to 3. It is thought that it is orientated along the thickness direction of a heat conductive sheet.
  • the lightness L * represented by the “L *” value in the L * a * b color system when aluminum nitride is contained in the heat conductive sheet and the surface of the heat conductive sheet is measured is 32. It was found that the pitch-based carbon fiber was oriented along the thickness direction of the heat conductive sheet and the heat conductivity in the thickness direction of the heat conductive sheet could be improved by being 0.5 or more.
  • Table 1 shows the measurement results of the thermal conductivity of the thermal conductive sheets obtained in Examples 1 to 6 and Comparative Examples 1 to 3. Evaluation of thermal conductivity was performed by a measurement method based on ASTM-D5470.
  • the heat conductive sheets obtained in Examples 1 to 6 have a heat conductivity in the thickness direction of the heat conductive sheet of 22.3 to 33.1 W / mK in the entire cross section of the heat conductive sheet. It was found that the thermal conductivity in the thickness direction was good. This is because the heat conductive sheets obtained in Examples 1 to 6 have the lightness represented by the “L *” value in the L * a * b color system when the surface of the heat conductive sheet is measured. Since L * was 32.5 or more, it is considered that the pitch-based carbon fibers were oriented along the thickness direction of the thermal conductive sheet, and the thermal conductivity in the thickness direction of the thermal conductive sheet could be improved. .
  • the thermal conductive sheets obtained in Comparative Examples 1 to 3 have a thermal conductivity of 20.2 W / mK or less, compared with the thermal conductive sheets obtained in Examples 1 to 6. Thus, it was found that the thermal conductivity in the thickness direction is not good. This is because the thermal conductive sheets obtained in Comparative Examples 1 to 3 do not contain aluminum nitride in the thermal conductive sheet, and the L * when the surface of the thermal conductive sheet is measured. This is presumably because the lightness L * represented by the “L *” value in the a * b color system is not 32.5 or higher.
  • the defect rate was evaluated based on the number of air bubbles entrained on the surface of the thermally conductive sheet or through holes in the thermally conductive sheet when the thermally conductive sheet was sliced from the cured silicone. .
  • the presence or absence of bubbles and whether or not the sheet has a through hole were determined by visually observing the cross section of the thermally conductive sheet.
  • the heat conductive sheet obtained in Comparative Example 1 had a high defect rate of 28% because bubbles were entrained on the surface and through holes were present in the sheet. This is presumably because the dispersibility of the silicone resin composition was poor because aluminum nitride was not contained in the heat conductive sheet.
  • the heat conductive sheet obtained in Comparative Example 3 has no bubbles entrained on the surface of the heat conductive sheet, and since there are no through holes in the heat conductive sheet, the defect rate is less than 5%. It was low. However, compared with Examples 1 to 6, the thermal conductivity was not good. This is presumably because the heat conductive sheet obtained in Comparative Example 3 did not contain aluminum nitride and the amount of alumina was too large.

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EP3412733A4 (en) * 2016-02-01 2019-10-09 Bando Chemical Industries, Ltd. HEAT-RESISTANT RESIN FORMING
JP6692512B1 (ja) * 2018-12-25 2020-05-13 富士高分子工業株式会社 熱伝導組成物及びこれを用いた熱伝導性シート
WO2020137086A1 (ja) * 2018-12-25 2020-07-02 富士高分子工業株式会社 熱伝導組成物及びこれを用いた熱伝導性シート
CN115141460A (zh) * 2021-03-30 2022-10-04 太阳油墨(苏州)有限公司 热固性树脂组合物、固化物以及电子部件
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EP3228590A4 (en) * 2014-12-02 2018-07-25 Sekisui Chemical Co., Ltd. Thermally-conductive sheet and method for producing same
EP3412733A4 (en) * 2016-02-01 2019-10-09 Bando Chemical Industries, Ltd. HEAT-RESISTANT RESIN FORMING
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JP6692512B1 (ja) * 2018-12-25 2020-05-13 富士高分子工業株式会社 熱伝導組成物及びこれを用いた熱伝導性シート
WO2020137086A1 (ja) * 2018-12-25 2020-07-02 富士高分子工業株式会社 熱伝導組成物及びこれを用いた熱伝導性シート
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CN115141460A (zh) * 2021-03-30 2022-10-04 太阳油墨(苏州)有限公司 热固性树脂组合物、固化物以及电子部件
CN115141460B (zh) * 2021-03-30 2023-09-01 太阳油墨(苏州)有限公司 热固性树脂组合物、固化物以及电子部件
WO2023238693A1 (ja) * 2022-06-08 2023-12-14 デクセリアルズ株式会社 積層体及びその製造方法
WO2023238692A1 (ja) * 2022-06-08 2023-12-14 デクセリアルズ株式会社 積層体及びその製造方法
WO2023238694A1 (ja) * 2022-06-08 2023-12-14 デクセリアルズ株式会社 積層体及びその製造方法

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